Layer-by-Layer technology to functionalize cellulose fibres and fibrils
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1 BiMaC Innovation Centre Day 29/01/2018 Layer-by-Layer technology to functionalize cellulose fibres and fibrils Andrew Marais
2 Outline Background Polyelectrolyte adsorption on fibres Layer-by-Layer functionalization of fibres Layer-by-Layer functionalization of nanofibres Conclusions and future perspectives 2
3 Background PhD dissertation (May 2015) BiMaC Innovation DLP5 Fibre Technology - Prof. Lars Wågberg Tailoring the interfibre joints properties, surface modification, paper mechanical properties 3
4 Background: life after BiMaC Innovation Postdoc (2 years) at Stanford University Wallenberg scholarship Prof. Yi Cui, Material Sciences BiMaC visitors! 4
5 Wood hierarchical structure Wood m Objective Surface modification of Fibres and Nanofibres Fibre µm-mm Nanofibre nm Cellulose Å 5
6 From wood to nanofibres Pulping - Bleaching Wood Ø Cellulose Ø Hemicellulose Ø Lignin Cellulose Nanofibres (CNF) Ø L a few µm Ø D 5 nm Ø High charge Fibres Ø L 2-5 mm Ø D 30 µm Homogenization 6
7 Outline Background Polyelectrolyte adsorption on fibres Layer-by-Layer functionalization of fibres Layer-by-Layer functionalization of nanofibres Conclusions and future perspectives 7
8 Polyelectrolyte adsorption Ø Adsorption on cellulose fibres ph Surface charge Salt concentration Porosity Entropy-driven 8
9 Adsorption of polyamines on fibres PAH (Polyallylamine) PVAm (Polyvinylamine) Ø ~2 mg/g ~50% increase in Tensile Index (PAH 56 KDa) 9
10 Interfibre joint strength Ø Increase in joint strength % Ø Distribution shifted towards stronger joints Median (MPa) Number of specimens Unmodified fibres 1.94 ± Modified fibres 2.28 ±
11 Interfibre contacts X-ray microtomography Contact area (µm 2 ) Number of contacts per mm fibre Unmodified 220 ± Modified 272 ±
12 Adsorption of polyamine monolayers Ø PAH and PVAm are efficient dry strength agents Ø Scalable, cheap, easy to handle Ø Microscopic mechanisms: Less weak joints / More strong joints Increased amount of joints Increased contact area 12
13 Outline Background Polyelectrolyte adsorption on fibres Layer-by-Layer functionalization of fibres Layer-by-Layer functionalization of nanofibres Conclusions and future perspectives 13
14 Polyelectrolyte multilayers Layer-by-Layer (LbL) technique Decher (1997), Science Advantages Parameters Applications Green Easy Cheap Versatile ph Salt concentration Optics Biomedicine Adhesion 14
15 Hyaluronic acid (HA) - LbL assemblies Dual Polarization Interferometry Application onto pulp fibres Ø Effect of salt Ø Superlinear growth 15
16 (PAH/HA) on fibres mechanical properties Ø Effect of salt Ø Tensile index and Strain at break increased by a factor of 3 16
17 (PAH/HA) Structure (AFM) Assembly in 10 mm NaCl 2x2 µm 2 z-range 30 nm Added salt Formation of a rough film Outermost layer - PAH : evening out effect - HA: roughening effect 17
18 Adhesive properties AFM colloidal probe (PAH/HA) 3 10 s contact Ø Influence of: Contact time - Number of layers - Outermost layer Ø Very strong wet adhesion over large separation distances 18
19 Explanation at the interfibre joint level Ø Anchoring of the first layer Charge interaction Penetration in the fibre wall (porous structure) Ø Mechanical properties of the LbL film (ductile) Intermixing of the layers within the film 19
20 Summary (PAH/HA) LbL on fibres Ø Nanostructures Rough film Ø Highly adhesive nm-thick films Ø Application on fibres for stretchable papers 3D packaging Scalable : LbL pilot scale on FEX, Innventia 20
21 Outline Background Polyelectrolyte adsorption on fibres Layer-by-Layer functionalization of fibres Layer-by-Layer functionalization of nanofibres Conclusions and future perspectives 21
22 CNF aerogels crosslinked with BTCA Freeze drying CNF gel (2 wt%) CNF gel + BTCA CNF aerogel Ø Water stability Ø Charge increase 22
23 5 mm Porosity 99 % Density 0.02 g/cm 3 Charge 2300 µeq/g 23
24 Aerogel functionalization by LbL Ø Dipping, spraying 24
25 25
26 Building 3D interdigitated devices 26
27 SEM images of the devices step by step Electrode 1 Electrode 1 - Separator Electrode 1 - Separator - Electrode 2 50 µm 2 µm Electrode 1 Separator Electrode 2 CNT (PEI/PAA) 30 CNT 27
28 Electrochemical characterization Ø No short-circuit! Ø Typical carbon supercapacitor behaviour Ø Concept validation 28
29 Test under compression 29
30 1 cm Ø Flexibility Ø Shape control Copper Hexacyanoferrate Ø Versatility 30
31 Conclusions Ø Paper mechanical properties tailored by LbL Strength, stretchability Fundamental studies showed effects on interfibre joints Ø Scalability Pilot scale trials Ø Development and functionalization of CNF porous materials Application for energy storage device 31
32 Future perspectives for LbL on cellulose Ø Versatility Wide range of applications Can serve most current hot topics Energy storage, health, functional textiles Ø Scalability Can target both mass production and high added value products 32
33 Acknowledgements BiMaC Innovation Wallenberg foundation Prof. Lars Wågberg Fibre Technology group You for listening 33
34 Quartz Crystal Microbalance with Dissipation Monitoring SiO 2, Au, (QCM-D) Cellulose Mainly used to study adsorption/attachment to surfaces in real time Quartz crystal Quartz crystal oscillating due to the piezoelectric effect Frequency: adsorbed mass Detectors for amplitude and frequency Slope: viscoelastic properties T = 1/f 0 ~ Driving voltage 6 Pulse relay Oscillation amplitude (V) Δf ΔD Pulses of driving voltage 1 0 t t :00:00 00:20:00 00:40:00 01:00:00 01:20:00 01:40:00 02:00:00 Progress time (hh:mm:ss) 2 1 Adsorbing polymer sample on crystal surface
35 Atomic Force Microscope (AFM)
36 DPI 36
37 PVAm From BASF; hydrolysis rate >90% 37
38 Polymer pka Mw (kda) PAH 9 15 ; 56 PVAm 45 ; 340 PEI 5,5 (2 ndary amine) 60 HA PAA 6,
39 3D (hybrid) battery Cathode Separator Anode CuHCF (PEI/PAA) 30 CNT 1 µm Copper Hexacyanoferrate (CuHCF) 1 µm Wessells et al., Nature Communications, Andrew Marais PhD defense - 22/05/2015
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